An innovative sampling approach combined with liquid chromatography-tandem mass spectrometry for the analysis of...

In this work, an innovative sampling and preconcentration method followed by analysis with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization (LC-ESI-MS/MS) was developed for the determination of different emerging pollutants (five anti-inflammatory drugs and one antibacterial agent) in water matrices. Thin-film microextraction blades, consisting of stainless steel blades with a coating made of divinylbenzene, have been employed. The blades, fixed onto a stainless steel support, were mounted on a laboratory stirrer with adjustable speed, immersed in water samples and eluted with methanol. The analytical procedure was developed, carefully optimizing stirring speed and extraction time. A good reproducibility among the blades was observed; quantitation limits at the ng L^-1 level were achieved. Calibration curves were constructed by applying the whole procedure to tap water samples, free from analytes, spiked with standards in the concentration range 0.01-2 μg L^-1 ; good linearity was obtained, with R² between 0.9984 and 0.9991. The optimized method was applied to tap and surface waters; two anti-inflammatory drugs were detected at the ng L^-1 level in surface water. In one sample, diclofenac and naproxen were measured at 26 ± 5 and 15 ± 1 ng L^-1 , respectively; only diclofenac was quantified in the other sample at 14 ± 3 ng L^-1 .